US2026049058A1PendingUtilityA1
Crystalline forms of picolinamide fungicide compound
Est. expiryMay 31, 2042(~15.8 yrs left)· nominal 20-yr term from priority
B01D 9/0036B01D 9/0018C07D 213/81
47
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Claims
Abstract
The present technology relates to processes useful for making crystalline S)-1,1-bis(4-fluorophenyl)propan-2-yl (3-acetoxy-4-methoxypicolinoyl)-L-alaninate (Compound I). Processes disclosed herein describe more stable, storage compatible preparations of Compound I. Also disclosed are preparations of Compound I which have fewer (trace) impurities.
Claims
exact text as granted — not AI-modifiedWe claim:
1 . A process for the preparation of a crystalline compound of the formula:
the process comprising:
distilling a mixture comprising: an aprotic organic solvent, a protic organic solvent, Compound I and seed Compound I.
2 . A process for the preparation of a crystalline compound of the formula:
the process comprising:
a. distilling a mixture comprising: an aprotic organic solvent and Compound I;
b. crystallizing Compound I from step a by creating a second mixture comprising: a protic organic solvent, Compound I and seed Compound I.
3 . The process of claim 1 wherein the aprotic organic solvent is dichloromethane.
4 . The process of claim 2 wherein the amount of dichloromethane in the mixture after step a is less than 1 wt % and greater than 0.01 wt % residual dichloromethane.
5 . The process of claim 2 wherein the amount of dichloromethane in the mixture after step a is less than 0.5 wt % and greater than 0.005 wt % residual dichloromethane.
6 . The process of claim 2 wherein a protic organic solvent is added to the mixture in step a.
7 . The process of claim 2 wherein the mixture after step a and before step b has a water content of less than 1000 ppm and greater than 50 ppm as analyzed by Karl Fisher method.
8 . The process of claim 2 wherein the mixture after step a and before step b has a water content of less than 300 ppm and greater than 0.1 ppm as analyzed by Karl Fisher method.
9 . The process of claim 2 wherein the amount of Compound I in the mixture after step a and before step b is less than 15 wt % and greater than 7 wt %.
10 . The process of claim 2 wherein the amount of Compound I in the mixture after step a and before step b is less than 15 wt % and greater than 10 wt %.
11 . The process of claim 2 wherein the amount of Compound I in the mixture after step a and before step b is less than 10 wt % and greater than 7 wt %.
12 . The process of claim 2 wherein the temperature during step a is performed in a range from about 60° C. to about 10° C.
13 . The process of claim 2 wherein the amount of seed Compound I is less than 50 wt % and greater than 15 wt %.
14 . The process of claim 2 wherein the amount of seed Compound I is less than 10 wt % and greater than 2 wt %.
15 . The process of claim 2 wherein the temperature during step b is performed in a range from about 50° C. to about 0° C.
16 . A crystalline polymorph of a compound of the formula:
17 . The polymorph of claim 16 wherein the polymorph is characterized by a powder X-ray diffraction pattern having at least the 2θ reflection positions:
2θ
5.97
10.69
14.71
16.99
19.41
23.21.
18 . The polymorph of claim 16 wherein the polymorph is characterized by a powder X-ray diffraction pattern having at least the 2θ reflection positions:
2θ
13.52
14.94
18.72
19.82
20.54
22.54
22.84.Join the waitlist — get patent alerts
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